EP0555110B2 - Process for thermochemical oxidation of nitrous oxide - Google Patents
Process for thermochemical oxidation of nitrous oxide Download PDFInfo
- Publication number
- EP0555110B2 EP0555110B2 EP93400042A EP93400042A EP0555110B2 EP 0555110 B2 EP0555110 B2 EP 0555110B2 EP 93400042 A EP93400042 A EP 93400042A EP 93400042 A EP93400042 A EP 93400042A EP 0555110 B2 EP0555110 B2 EP 0555110B2
- Authority
- EP
- European Patent Office
- Prior art keywords
- nitrous oxide
- flame
- dinitrogen oxide
- oxide
- oxidation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/24—Nitric oxide (NO)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/36—Nitrogen dioxide (NO2, N2O4)
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
Definitions
- the present invention relates to a method of thermochemical decomposition of nitrous oxide.
- Nitric oxidation of various organic substrates releases various nitrogen oxides, some of which may be easily recovered or destroyed such as nitric oxide, nitrogen dioxide, or tetroxide dinitrogen. But other nitrogen oxides, especially dinitrogen monoxide, are not directly recyclable.
- N 2 O nitrous oxide at room temperature, is a stable gas, not substantially combining with molecular oxygen, and resistant to the action of conventional oxidants. At high temperatures, it is a remarkable oxidizer yielding easily its oxygen and releasing molecular nitrogen with a strong release of heat.
- Some chemical reactions such as nitric oxidation of acetaldehyde to glyoxal or oxidation Nitrate of cyclohexanone in adipic acid release large amounts of nitrous oxide.
- the process according to the present invention is a thermochemical oxidation process in which the nitrous oxide is treated with flame, then the products of general formula (I) formed are recovered.
- the flame is obtained by conventional combustion of a mixture of oxidizing and combustible gases selected from the group consisting of molecular oxygen, nitrous oxide, natural gas, associated lower alkanes generally to a ballast constituted by molecular nitrogen.
- the gaseous mixture containing the nitrous oxide is injected, either into the flame or into the gases hot from the flame. In the latter case, the injection is called post combustion injection.
- the above process is particularly applicable to gas mixtures, in particular effluents industrial plants contain nitrous oxide.
- the process according to the invention consumes the entire nitrous oxide. Indeed the gases, after flame treatment, virtually no longer contain nitrous oxide. It is thought that temperature of the flame, the nitrous oxide decomposes in particular into atomic oxygen, into nitric oxide and molecular nitrogen.
- the process according to the present invention can advantageously be carried out continuously in a furnace equipped with a burner, one or more confinement chambers, and a device for injecting the effluent to be treated.
- the gases are cooled to the temperature then the products of general formula (I) are recovered, advantageously by absorption in a washing tower in which circulates dilute nitric acid.
- the oven used in these examples is a cylindrical, vertical oven with an internal diameter of 1300 mm and a height of 3500 mm. It has a power of 1 Mw and is lined with refractory material.
- the burner is turbulence adjustable element, named swirl, type polycombustible double air inlet.
- the containment chambers three in number, are cylindrical, vertical, filled with refractory: the top element is equipped with a burner, the quarl, the ignition device and the detection cell flame; the middle element contains an injection device with alumina tubes embedded in the material refractory and the bottom element is simple.
- the set of containment chambers measures 1400 mm height and has a diameter less than 450 mm.
- the flow rates of the gases are determined, either with a rotameter, either with a volumetric meter, or finally, with a venturi.
- the gases, after reaction, are analyzed with an infrared absorption analyzer for carbon monoxide, carbon dioxide and nitrous oxide, and with a paramagnetic analyzer for oxygen.
- the gases of general formula (I) are determined by acidimetry after oxidation with oxygen, then with hydrogen peroxide.
- the gas flow rates are expressed in cubic meters per hour at atmospheric pressure and at 20 ° C.
- the concentration of the various gases after reaction is expressed in percentages by volume except for the unconverted nitrous oxide which is expressed in ppm by volume.
- the flame is produced by burning natural gas in air.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
La présente invention concerne un procédé de décomposition thermochimique de l'oxyde de diazote.The present invention relates to a method of thermochemical decomposition of nitrous oxide.
L'oxydation nitrique de divers substrats organiques libère divers oxydes d'azote dont certains peuvent être aisément valorisés ou détruits tels que le monoxyde d'azote, le dioxyde d'azote, ou le tétraoxyde diazote. Mais d'autres oxydes d'azote, notamment le monoxyde de diazote, ne sont pas directement recyclables.Nitric oxidation of various organic substrates releases various nitrogen oxides, some of which may be easily recovered or destroyed such as nitric oxide, nitrogen dioxide, or tetroxide dinitrogen. But other nitrogen oxides, especially dinitrogen monoxide, are not directly recyclable.
L'oxyde de diazote N2O, à la température ambiante, est un gaz stable, ne se combinant pratiquement pas à l'oxygène moléculaire, et résistant bien à l'action des oxydants classiques. A hautes températures, c'est un comburant remarquable cédant facilement son oxygène et libérant de l'azote moléculaire avec un fort dégagement de chaleur.N 2 O nitrous oxide, at room temperature, is a stable gas, not substantially combining with molecular oxygen, and resistant to the action of conventional oxidants. At high temperatures, it is a remarkable oxidizer yielding easily its oxygen and releasing molecular nitrogen with a strong release of heat.
Certaines réactions chimiques telles que l'oxydation nitrique de l'acétaldéhyde en glyoxal ou l'oxydation nitrique de la cyclohexanone en acide adipique libèrent de grandes quantités d'oxyde de diazote.Some chemical reactions such as nitric oxidation of acetaldehyde to glyoxal or oxidation Nitrate of cyclohexanone in adipic acid release large amounts of nitrous oxide.
Il est donc d'un grand intérêt industriel de pouvoir transformer cet oxyde de diazote en des oxydes d'azote de degré d'oxydation supérieur en vue de leur valorisation notamment pour la fabrication d'acide nitrique.It is therefore of great industrial interest to be able to transform this nitrous oxide into oxides. nitrogen with a higher degree of oxidation for recovery, in particular for acid production nitric.
Il est connu par la demande de brevet japonais N° 61-257.940, un procédé de décomposition thermique permettant de transformer en oxyde d'azote les sous-produits gazeux (N2O, NO, NO2) formés lors de l'oxydation nitrique de la cyclohexanone et/ou du cyclohexanol en acide adipique, procédé qui doit être mis en oeuvre impérativement dans un réacteur piston après avoir abaissé la somme des concentrations en NO et en NO2 dans le mélange gazeux de départ à moins de 10 %.It is known from Japanese Patent Application No. 61-257,940, a thermal decomposition process for converting the gaseous by-products (N 2 O, NO, NO 2 ) formed in nitric oxidation into nitrogen oxide. cyclohexanone and / or cyclohexanol to adipic acid, which method must be implemented imperatively in a piston reactor after lowering the sum of the concentrations of NO and NO 2 in the starting gas mixture to less than 10%.
Or, afin de s'affranchir de cette double exigence qui nécessite une technologie complexe, la demanderesse
a découvert avec étonnement un procédé permettant de transformer l'oxyde de diazote en produits
de formule (I)
Le procédé selon la présente invention est un procédé d'oxydation thermochimique dans lequel on traite à la flamme l'oxyde de diazote, puis l'on récupère les produits de formule générale (I) formés.The process according to the present invention is a thermochemical oxidation process in which the nitrous oxide is treated with flame, then the products of general formula (I) formed are recovered.
La flamme est obtenue par combustion classique d'un mélange de gaz comburants et combustibles choisis dans le groupe constitué par l'oxygène moléculaire, l'oxyde de diazote, le gaz naturel, les alcanes inférieurs associés généralement à un ballast constitué par de l'azote moléculaire.The flame is obtained by conventional combustion of a mixture of oxidizing and combustible gases selected from the group consisting of molecular oxygen, nitrous oxide, natural gas, associated lower alkanes generally to a ballast constituted by molecular nitrogen.
Le mélange gazeux contenant l'oxyde de diazote est injecté, soit dans la flamme, soit dans les gaz chauds issus de la flamme. Dans ce dernier cas, l'injection est appelée injection en post combustion.The gaseous mixture containing the nitrous oxide is injected, either into the flame or into the gases hot from the flame. In the latter case, the injection is called post combustion injection.
Le procédé ci-dessus est particulièrement applicable à des mélanges gazeux, notamment des effluents industriels renferment de l'oxyde de diazote.The above process is particularly applicable to gas mixtures, in particular effluents industrial plants contain nitrous oxide.
Il est connu que le monoxyde d'azote, NO, à la température ambiante, au contact d'oxygène, s'oxyde quantitativement, immédiatement et exothermiquement en dioxyde d'azote, NO2. Mais cette réaction est équilibrée et il est admis qu'à la pression atmosphérique, au dessus de 620°C, un mélange d'oxygène et de NO peut rester sans donner lieu à la moindre réaction. Par contre, à la température ambiante, la réaction est complète et il n'existe pratiquement plus de NO. Il est également connu que le dioxyde d'azote se dimérise en tétraoxyde de diazote et que cette dimérisation est d'autant plus complète que la température est plus basse. A la température et à la pression ambiantes, le dioxyde d'azote est presque entièrement dimérisé en N2O4 se dissolvant très rapidement dans l'eau en donnant de l'acide nitrique et de l'acide nitreux.It is known that nitrogen monoxide, NO, at room temperature, in contact with oxygen, oxidizes quantitatively, immediately and exothermically to nitrogen dioxide, NO 2 . But this reaction is balanced and it is admitted that at atmospheric pressure, above 620 ° C, a mixture of oxygen and NO can remain without giving rise to the slightest reaction. By cons, at room temperature, the reaction is complete and there is virtually no NO. It is also known that nitrogen dioxide dimerizes into dinitrogen tetroxide and that this dimerization is all the more complete as the temperature is lower. At ambient temperature and pressure, nitrogen dioxide is almost completely dimerized to N 2 O 4 , dissolving very rapidly in water to give nitric acid and nitrous acid.
Le procédé selon l'invention, consomme entièrement l'oxyde de diazote. En effet les gaz, après traitement à la flamme , ne contiennent pratiquement plus d'oxyde de diazote. On pense qu'à la température de la flamme, l'oxyde de diazote se décompose notamment en oxygène atomique, en monoxyde d'azote et en azote moléculaire.The process according to the invention consumes the entire nitrous oxide. Indeed the gases, after flame treatment, virtually no longer contain nitrous oxide. It is thought that temperature of the flame, the nitrous oxide decomposes in particular into atomic oxygen, into nitric oxide and molecular nitrogen.
Le procédé selon la présente invention peut être avantageusement mis en oeuvre en continu dans un four équipé d'un brûleur, d'une ou plusieurs chambres de confinement, et d'un dispositif d'injection de l'effluent à traiter. A la sortie de la ou des chambres de confinement, les gaz sont refroidis à la température ambiante, puis les produits de formule générale (I) sont récupérés, avantageusement par absorption dans une tour de lavage dans laquelle circule de l'acide nitrique dilué.The process according to the present invention can advantageously be carried out continuously in a furnace equipped with a burner, one or more confinement chambers, and a device for injecting the effluent to be treated. At the outlet of the confinement chamber or chambers, the gases are cooled to the temperature then the products of general formula (I) are recovered, advantageously by absorption in a washing tower in which circulates dilute nitric acid.
Il est avantageux que le procédé de la présente invention soit mis en oeuvre à la pression atmosphérique.It is advantageous that the process of the present invention is carried out at atmospheric pressure.
Les exemples suivants illustrent le procédé de la présente invention. The following examples illustrate the process of the present invention.
Le four utilisé dans ces exemples est un four cylindrique, vertical, d'un diamètre intérieur de 1300 mm et d'une hauteur de 3500 mm. Il présente une puissance de 1 Mw et il est garni de matière réfractaire. Le brûleur est à turbulence à élément réglable, nommé swirl, du type polycombustible à double entrée d'air. Les chambres de confinement, au nombre de trois, sont cylindriques, verticales, garnies de réfractaire : l'élément haut est équipé d'un brûleur, de l'ouvreau, du dispositif d'allumage et de la cellule de détection de flamme ; l'élément du milieu contient un dispositif d'injection à tubes d'alumine noyés dans la matière réfractaire et l'élément du bas est simple. L'ensemble des chambres de confinement mesure 1400 mm de hauteur et a un diamètre inférieur à 450 mm. Les débits des gaz sont déterminés, soit avec un rotamètre, soit avec un compteur volumétrique, soit enfin, avec un venturi. Les gaz, après réaction, sont analysés avec un analyseur à absorption infrarouge pour l'oxyde de carbone, le dioxyde de carbone et l'oxyde de diazote, et avec un analyseur paramagnétique pour l'oxygène. Les gaz de formule générale (I) sont dosés par acidimétrie après oxydation avec de l'oxygène, puis avec du peroxyde d'hydrogène.The oven used in these examples is a cylindrical, vertical oven with an internal diameter of 1300 mm and a height of 3500 mm. It has a power of 1 Mw and is lined with refractory material. The burner is turbulence adjustable element, named swirl, type polycombustible double air inlet. The containment chambers, three in number, are cylindrical, vertical, filled with refractory: the top element is equipped with a burner, the quarl, the ignition device and the detection cell flame; the middle element contains an injection device with alumina tubes embedded in the material refractory and the bottom element is simple. The set of containment chambers measures 1400 mm height and has a diameter less than 450 mm. The flow rates of the gases are determined, either with a rotameter, either with a volumetric meter, or finally, with a venturi. The gases, after reaction, are analyzed with an infrared absorption analyzer for carbon monoxide, carbon dioxide and nitrous oxide, and with a paramagnetic analyzer for oxygen. The gases of general formula (I) are determined by acidimetry after oxidation with oxygen, then with hydrogen peroxide.
Le rendement de destruction de l'oxyde de diazote est calculé comme suit :
Le rendement de la conversion de N2O en NOx (exprimé en N2O) est calculé comme suit :
- [N2O]* :
- concentration en oxyde de diazote après réaction
- [N2O] :
- concentration en oxyde de diazote avant réaction
- [NOx]* :
- concentration en NOx (exprimé en NO2) après réaction
- DT :
- débit total des gaz entrant dans le réacteur
- DE :
- débit de l'effluent gazeux.
- NM :
- non mesurable ; concentration inférieure ou égale à 100 ppmv.
- [N 2 O] *:
- concentration of dinitrogen oxide after reaction
- [N 2 O]:
- concentration of dinitrogen oxide before reaction
- [NO x ] *:
- NO x concentration (expressed as NO 2 ) after reaction
- DT:
- total flow of gases entering the reactor
- FROM:
- flow rate of the gaseous effluent.
- NM:
- Unmeasurable ; concentration less than or equal to 100 ppmv.
Les débits des gaz sont exprimés en mètre cube par heure à la pression atmosphérique et à 20 °C.The gas flow rates are expressed in cubic meters per hour at atmospheric pressure and at 20 ° C.
La concentration des divers gaz après réaction est exprimée en pourcentages volumiques sauf pour l'oxyde de diazote non transformé qui est exprimé en ppm volumique.The concentration of the various gases after reaction is expressed in percentages by volume except for the unconverted nitrous oxide which is expressed in ppm by volume.
La flamme est produite par la combustion de gaz naturel dans de l'air. The flame is produced by burning natural gas in air.
Les exemples 1 à 9 sont rassemblés dans le tableau 1.
Claims (3)
- Process for the thermochemical decomposition of dinitrogen oxide to products of formula (I)
- Process according to claim 1, characterized in that the dinitrogen oxide to be decomposed is one of the components of a gas mixture.
- Process according to claim 2, characterized in that the gas mixture is an industrial effluent.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9201413 | 1992-02-07 | ||
| FR9201413A FR2687138A1 (en) | 1992-02-07 | 1992-02-07 | PROCESS FOR THERMOCHEMICAL OXIDATION OF DIAZOTE OXIDE |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0555110A1 EP0555110A1 (en) | 1993-08-11 |
| EP0555110B1 EP0555110B1 (en) | 1995-08-09 |
| EP0555110B2 true EP0555110B2 (en) | 2005-02-02 |
Family
ID=9426449
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP93400042A Expired - Lifetime EP0555110B2 (en) | 1992-02-07 | 1993-01-11 | Process for thermochemical oxidation of nitrous oxide |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US5429811A (en) |
| EP (1) | EP0555110B2 (en) |
| JP (1) | JP3877785B2 (en) |
| KR (1) | KR100237981B1 (en) |
| CA (1) | CA2088873C (en) |
| DE (1) | DE69300331T3 (en) |
| FR (1) | FR2687138A1 (en) |
| RU (1) | RU2104922C1 (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2709748B1 (en) * | 1993-09-10 | 1995-10-27 | Rhone Poulenc Chimie | Process for the plasmachemical transformation of N2O into NOx and / or its derivatives. |
| US5472680A (en) * | 1994-01-26 | 1995-12-05 | E. I. Du Pont De Nemours And Company | Production of NO from N2 O |
| DE19533715A1 (en) * | 1995-09-12 | 1997-03-13 | Basf Ag | Process for removing nitrogen oxides from a gas stream containing them |
| WO1999025461A1 (en) * | 1997-11-18 | 1999-05-27 | Asahi Kasei Kogyo Kabushiki Kaisha | Method and device for global warming prevention |
| DE19902109A1 (en) | 1999-01-20 | 2000-07-27 | Basf Ag | Process for thermal N¶2¶O decomposition |
| CN100431670C (en) * | 2006-04-07 | 2008-11-12 | 北京布鲁斯盖环保科技发展有限公司 | Energy-saving method for denitrogenation of horizontal chained coal fired boiler |
| US10723624B2 (en) | 2017-12-05 | 2020-07-28 | Ascend Performance Materials Operations Llc | Process for preparation of nitrogen oxides and nitric acid from nitrous oxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB325475A (en) † | 1928-11-12 | 1930-02-12 | Ig Farbenindustrie Ag | Improvements in the manufacture and production of nitrous oxide from ammonia |
| JPS61257940A (en) † | 1985-05-13 | 1986-11-15 | Asahi Chem Ind Co Ltd | Production of dicarboxylic acid |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3797415A (en) * | 1972-10-30 | 1974-03-19 | J Young | Incinerator with a plurality of outer walls and a hollow grate |
| JPS60257940A (en) * | 1984-06-06 | 1985-12-19 | Toyota Motor Corp | Production of cam shaft |
| NO165539C (en) * | 1988-09-16 | 1991-02-27 | Norsk Hydro As | METHOD OF REDUCING NITROGEN OXIDE. |
| US5133950A (en) * | 1990-04-17 | 1992-07-28 | A. Ahlstrom Corporation | Reducing N2 O emissions when burning nitrogen-containing fuels in fluidized bed reactors |
| US5043150A (en) * | 1990-04-17 | 1991-08-27 | A. Ahlstrom Corporation | Reducing emissions of N2 O when burning nitrogen containing fuels in fluidized bed reactors |
| US5200162A (en) * | 1992-04-01 | 1993-04-06 | Uop | Process for N2 O decomposition |
-
1992
- 1992-02-07 FR FR9201413A patent/FR2687138A1/en active Granted
-
1993
- 1993-01-11 DE DE69300331T patent/DE69300331T3/en not_active Expired - Lifetime
- 1993-01-11 EP EP93400042A patent/EP0555110B2/en not_active Expired - Lifetime
- 1993-02-03 JP JP04041393A patent/JP3877785B2/en not_active Expired - Lifetime
- 1993-02-05 RU RU93004477A patent/RU2104922C1/en not_active IP Right Cessation
- 1993-02-05 US US08/016,141 patent/US5429811A/en not_active Expired - Lifetime
- 1993-02-05 CA CA002088873A patent/CA2088873C/en not_active Expired - Lifetime
- 1993-02-06 KR KR1019930001629A patent/KR100237981B1/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB325475A (en) † | 1928-11-12 | 1930-02-12 | Ig Farbenindustrie Ag | Improvements in the manufacture and production of nitrous oxide from ammonia |
| JPS61257940A (en) † | 1985-05-13 | 1986-11-15 | Asahi Chem Ind Co Ltd | Production of dicarboxylic acid |
Non-Patent Citations (4)
| Title |
|---|
| "Aspects physiques et chimiques de la Combustion" (1976) editions echnip, G. de Soete, A. Feugier † |
| Note technique de la NASA publiée en Mai 1963. † |
| Note technique de la NASA publiée en Novembre 1962. † |
| SR 1 Pep Report Nr. 54 B (1987) p. 45-65 † |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3877785B2 (en) | 2007-02-07 |
| EP0555110A1 (en) | 1993-08-11 |
| DE69300331D1 (en) | 1995-09-14 |
| DE69300331T2 (en) | 1996-01-04 |
| KR100237981B1 (en) | 2000-03-02 |
| US5429811A (en) | 1995-07-04 |
| CA2088873C (en) | 2003-07-08 |
| EP0555110B1 (en) | 1995-08-09 |
| FR2687138B1 (en) | 1994-07-13 |
| KR930017810A (en) | 1993-09-20 |
| DE69300331T3 (en) | 2005-11-17 |
| RU2104922C1 (en) | 1998-02-20 |
| FR2687138A1 (en) | 1993-08-13 |
| CA2088873A1 (en) | 1993-08-08 |
| JPH05339003A (en) | 1993-12-21 |
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